HRID1493187
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A reaction mixture containing phenyl(4-piperidinyl)methanone (20.5 g, 0.108 mol), K2CO3 (33.17 g, 0.18 mol), potassium iodide (0.2 g) and 2-bromoethyl benzene (22.2 g, 0.12 mol, 16.4 ml) in toluene (250 ml) was stirred at reflux temperature for 66 h. The reaction mixture was filtered and the filtrate concentrated to a residue which was dissolved in dry Et2O (500 ml) and treated dropwise with a solution of HCl (0.11 mol) in EtOAc. The resultant precipitate was recrystallized from EtOH:CH3OH, 4:1 (500 ml ) to give phenyl[1-(2-phenylethyl)-4-piperidinyl]-methanone hydrochloride, mp 258°-260° C.
WORKUP
后处理
- temperatureat reflux temperature for 66 h
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate concentrated to a residue which
- dissolutionwas dissolved in dry Et2O (500 ml)
- customThe resultant precipitate was recrystallized from EtOH